CN117626421A - Method for reducing stress in CVD single crystal diamond growth process - Google Patents
Method for reducing stress in CVD single crystal diamond growth process Download PDFInfo
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- CN117626421A CN117626421A CN202311753872.0A CN202311753872A CN117626421A CN 117626421 A CN117626421 A CN 117626421A CN 202311753872 A CN202311753872 A CN 202311753872A CN 117626421 A CN117626421 A CN 117626421A
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- 239000013078 crystal Substances 0.000 title claims abstract description 132
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 111
- 239000010432 diamond Substances 0.000 title claims abstract description 111
- 238000000034 method Methods 0.000 title claims abstract description 46
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000011889 copper foil Substances 0.000 claims abstract description 33
- 238000005530 etching Methods 0.000 claims abstract description 16
- 238000003763 carbonization Methods 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 238000007747 plating Methods 0.000 claims abstract description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 16
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 14
- 229910052750 molybdenum Inorganic materials 0.000 claims description 14
- 239000011733 molybdenum Substances 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 13
- 238000000151 deposition Methods 0.000 claims description 13
- 239000011248 coating agent Substances 0.000 claims description 12
- 230000008021 deposition Effects 0.000 claims description 11
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 238000000259 microwave plasma-assisted chemical vapour deposition Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 2
- 238000007781 pre-processing Methods 0.000 claims description 2
- 230000003746 surface roughness Effects 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 238000004544 sputter deposition Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 238000003466 welding Methods 0.000 abstract description 4
- 238000009825 accumulation Methods 0.000 abstract description 3
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 2
- 230000003287 optical effect Effects 0.000 description 7
- 238000001237 Raman spectrum Methods 0.000 description 6
- 230000017525 heat dissipation Effects 0.000 description 5
- 238000001069 Raman spectroscopy Methods 0.000 description 4
- 238000010000 carbonizing Methods 0.000 description 4
- 238000000879 optical micrograph Methods 0.000 description 4
- 238000005554 pickling Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000005539 carbonized material Substances 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000009172 bursting Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for reducing stress in the growth process of CVD monocrystal diamond, which comprises the following steps: (1) cleaning a single crystal diamond seed crystal and a copper foil assembly; (2) Etching the non-growth surface of the single crystal diamond seed crystal; (3) Plating a metal Mo layer on the surface of the single crystal diamond seed etching surface; (4) Performing plasma surface carbonization treatment to generate a metal carbide layer; (5) Solidifying the treated monocrystalline diamond seed crystal and the metal copper foil pair Ji Gaowen, and welding and bonding by using a chemical vapor deposition furnace; (6) obtaining low stress single crystal diamond by growth. The invention aims to stabilize heat transfer between a single crystal diamond seed crystal and a sample growth table, reduce the growth temperature gradient of the surface of the single crystal diamond and reduce stress accumulation in the growth process of the CVD single crystal diamond.
Description
Technical Field
The invention belongs to the technical field of inorganic nonmetallic material manufacturing, and particularly relates to a method for reducing stress in a CVD monocrystal diamond growth process.
Background
Diamond is known to be the hardest material in nature, and has the properties of the highest thermal conductivity, the highest sound wave transmission speed, the largest young's modulus, the widest optical transmission frequency band, and the like in nature. Because of such many excellent properties, it plays an extremely important role in various high-tech fields such as precision machining, high-frequency communication, military field, aerospace and the like, the diamond synthesized by the conventional HPHT is yellow to dark yellow, the defect density is higher, the overall quality is relatively poor, the optical performance and the electrical performance of the semiconductor are seriously affected, and the application of the semiconductor in the high-tech fields such as aerospace, wide forbidden band semiconductors and the like is greatly limited. Compared with the HPHT synthesis method, the CVD method has the advantages of safe and simple synthesis equipment, larger synthesized diamond area, better crystal quality, lower synthesis cost, controllable doping and the like, and is currently considered as the diamond synthesis method with the most industrial application prospect.
When growing single crystal diamond by CVD, a diamond seed crystal is required to be maintained at a relatively stable and appropriate temperature to stably grow high quality single crystal diamond. Meanwhile, as the difference of heat conductivity coefficient, thermal expansion coefficient and the like between the diamond seed crystal and the molybdenum support bearing the seed crystal is larger, the phenomenon that the seed crystal moves or even drifts easily occurs during the temperature rising period, the phenomenon can change the position of the diamond seed crystal, and the uneven or unstable temperature of the diamond seed crystal is caused, so that the growth quality of single crystal diamond is affected, the appearance of the grown single crystal diamond is irregular, as shown in fig. 6, meanwhile, the internal stress is too large, the problem of cracking easily occurs when the diamond is applied to a tool, and the service life of the diamond is affected.
In order to prevent the seed from shifting, a method is sought that can fix the position of the seed while increasing the thermal conductivity between the seed and the molybdenum holder carrying the seed. The common method is a welding method, but welding media are difficult to find by the welding method, and most of the media are poor in compatibility with diamond, so that a diamond treatment method which has good compatibility with diamond and can effectively ensure heat dissipation between a seed crystal and a sample stage is needed.
Disclosure of Invention
The invention aims to provide a method for stably and uniformly radiating heat between a CVD single crystal diamond and a sample stage in the growth process.
The invention also provides a method for reducing stress in the growth process of the CVD single crystal diamond.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention discloses a method for reducing stress in the growth process of CVD single crystal diamond, which is characterized by comprising the following steps:
(1) Cleaning
Cleaning the single crystal diamond seed crystal to be treated and the heat conduction copper foil, and drying to remove impurities; the single crystal diamond seed crystal is flaky, the size is not particularly required, and the thickness of the copper foil is 20-150 microns;
(2) Seed etching
Etching and preprocessing the monocrystalline diamond seed crystal obtained in the step (1) in an oxyhydrogen plasma environment to obtain monocrystalline diamond seed crystal with larger surface roughness;
(3) Coating film
Plating molybdenum on the single crystal diamond seed crystal obtained in the step (2) through a plating process, and forming a metal layer on the diamond-shaped surface; the thickness of the metal layer is 0.1-1 micron;
(4) Carbonization treatment
Carrying out surface carbonization treatment on the single crystal diamond seed crystal plated with the molybdenum layer obtained in the step (3) in a hydrogen and methane plasma atmosphere, so that a metal carbide layer is generated on the surface of the single crystal diamond seed crystal plated with the molybdenum layer;
(5) Bonding
And (3) bonding the surface of the monocrystalline diamond seed crystal with the metal carbide layer obtained in the step (4) with the copper foil of the heat conducting layer in a plasma environment by a sample stage to obtain the monocrystalline diamond seed crystal bonded with the heat conducting copper foil.
(6) Deposition growth
And (3) placing the monocrystalline diamond seed crystal obtained in the step (5) into MPCVD equipment, and carrying out monocrystalline diamond deposition at high temperature to obtain the low-stress monocrystalline diamond under the same technological conditions.
Preferably, in the step (1), monocrystalline diamond seeds are placed in aqua regia for 2 hours in a water bath at 80 ℃, then the seeds and the heat conduction copper foil after pickling are respectively cleaned in acetone and absolute ethyl alcohol for 20 minutes in an ultrasonic manner, and then the seeds and the heat conduction copper foil are cleaned in pure water for 5 minutes and are placed in an oven for drying;
preferably, in the step (2), the single crystal diamond seed crystal is etched in an oxyhydrogen plasma environment, and the etching time t1 is more than or equal to 1h and less than or equal to 3h.
Preferably, the step (3) is a magnetron sputtering coating process.
Preferably, the magnetron sputtering coating is performed under the vacuum condition that the pressure is not more than 0.001Pa, the magnetron sputtering time is t, t2 is not more than 10min and not more than 15min, and the magnetron sputtering power is 100W.
Preferably, the carbonization treatment temperature in the step (4) is 700-800 ℃, the methane flow is 1-8% of the hydrogen volume flow, and the carbonization time is 0.5-2 h.
Preferably, the sample stage in the step (5) is bonded in a plasma environment at 900-1000 ℃ for not less than 1h.
Preferably, the single crystal diamond deposition temperature in step (6) is 850-950 ℃ and the deposition time is about 72-120h.
Compared with the prior art, the invention has the beneficial effects that:
by etching the surface of the seed crystal, the roughness of the bond and the surface can be effectively improved, and the contact area and the adhesive force of the plating layer and the single crystal diamond seed crystal are increased.
The metal carbide diffusion coating formed by plasma high-temperature surface carbonization treatment has better compatibility with diamond seed crystals, and simultaneously has better compatibility with copper foil, thereby establishing good connection between the diamond seed crystals and the copper foil and improving the heat conduction effect.
Through good bonding of seed crystal, copper foil and sample platform, increase its heat conduction ability, guarantee the even stability of seed crystal temperature during growth, can produce the single crystal diamond that the shape is leveled, and the internal stress is low, reduces the problem occurrence probability of bursting apart when single crystal diamond uses, further improves single crystal diamond's life in various instruments.
The heat transfer between the monocrystalline diamond seed crystal and the sample growth table is stabilized, the growth temperature gradient of the surface of the monocrystalline diamond is reduced, the defect accumulation caused by local temperature unevenness in the growth process of the CVD monocrystalline diamond is reduced, and then the stress accumulation in the monocrystalline diamond is reduced.
Drawings
FIG. 1 is a schematic diagram of the key and timing of the present invention;
FIG. 2 is an optical micrograph of a single crystal diamond seed after etching;
FIG. 3 is an optical micrograph of a molybdenum-coated single crystal diamond;
FIG. 4 is an optical micrograph of the carbonized material;
FIG. 5 is an XRD pattern after carbonization;
FIG. 6 is an optical photograph of a single crystal diamond grown prior to improving heat dissipation conditions
FIG. 7 is an optical photograph of single crystal diamond grown using a process according to an embodiment of the present invention;
FIG. 8 is an optical photograph of single crystal diamond grown using the process of example two of the present invention;
FIG. 9 is a comparison of Raman spectra of single crystal diamond grown prior to improving heat dissipation conditions;
FIG. 10 is a comparison of Raman spectra of single crystal diamond grown by a process according to an embodiment of the invention;
FIG. 11 is a comparison of Raman spectra of single crystal diamond grown by the process of example two of the present invention.
Description of the embodiments
The invention is further illustrated by the following examples, which are not intended to be limiting.
Examples
(1) Cleaning:
placing monocrystalline diamond seed crystal in aqua regia at 80 ℃ for 2 hours in water bath, respectively ultrasonically cleaning the seed crystal and the heat conduction copper foil in acetone and absolute ethyl alcohol for 20 minutes after pickling, cleaning the seed crystal and the heat conduction copper foil in pure water for 5 minutes, and placing the seed crystal and the heat conduction copper foil in an oven for drying; the single crystal diamond seed crystal is flaky, the size has no specific requirement, the thickness of the copper foil is 20 microns, and the specification of the copper foil is slightly larger than the size of the seed crystal in accordance with the seed crystal;
(2) Seed crystal etching:
placing the dried seed crystal into MPCVD equipment, and etching for 2 hours at 900 ℃ in an oxyhydrogen plasma environment, wherein the flow rate of hydrogen is 300sccm and the flow rate of oxygen is 2sccm; the etching of the seed surface is described with reference to fig. 2.
(3) Coating:
taking etched seed crystal, performing magnetron sputtering for 15min under the vacuum condition that the pressure is not more than 0.001Pa, wherein the power of the magnetron sputtering is 100W, and depositing to obtain single crystal diamond seed crystal plated with metallic molybdenum; the surface condition after coating can be referred to as figure 3.
(4) Carbonizing:
placing the seed crystal coating surface after coating on a sample stage of MPCVD equipment, carbonizing in a hydrogen and methane plasma atmosphere for 0.5h at 800 ℃, wherein the flow rate of the hydrogen is 300sccm, and the flow rate of the methane is 12sccm; FIG. 4 is an optical micrograph of the carbonized material; FIG. 5 is an XRD pattern after carbonization;
(5) Bonding:
the molybdenum table, the copper foil and the carbonized diamond are sequentially placed in MPCVD equipment from bottom to top, reference is made to figure 1, wherein the carbonized layer is contacted with the copper foil, and bonding is carried out for 1.5 hours at 1000 ℃ in a plasma environment, so that the monocrystalline diamond seed crystal bonded with the heat-conducting copper foil can be obtained and can be used for growing low-stress monocrystalline diamond.
(6) Deposition and growth:
and (3) placing the bonded monocrystalline diamond seed crystal into an MPCVD device, and carrying out monocrystalline diamond deposition at 850-950 ℃ for 72 hours to obtain the low-stress monocrystalline diamond under the same technological conditions.
Examples
(1) Cleaning:
placing monocrystalline diamond seed crystal in aqua regia at 80 ℃ for 2 hours in water bath, respectively ultrasonically cleaning the seed crystal and the heat conduction copper foil in acetone and absolute ethyl alcohol for 20 minutes after pickling, cleaning the seed crystal and the heat conduction copper foil in pure water for 5 minutes, and placing the seed crystal and the heat conduction copper foil in an oven for drying; the single crystal diamond seed crystal is flaky, the size has no specific requirement, the thickness of the copper foil is 20 microns, and the specification of the copper foil is slightly larger than the size of the seed crystal in accordance with the seed crystal;
(2) Seed crystal etching:
placing the dried seed crystal into MPCVD equipment, and etching for 3 hours at 850 ℃ in an oxyhydrogen plasma environment, wherein the flow rate of hydrogen is 300sccm and the flow rate of oxygen is 2sccm;
(3) Coating:
taking etched seed crystal, performing magnetron sputtering for 15min under the vacuum condition that the pressure is not more than 0.001Pa, wherein the power of the magnetron sputtering is 100W, and depositing to obtain single crystal diamond seed crystal plated with metallic molybdenum;
(4) Carbonizing:
placing the seed crystal coating surface after coating on a sample stage of MPCVD equipment, carbonizing in a methane plasma atmosphere for 2 hours at 700 ℃, wherein the flow rate of hydrogen used is 300sccm, and the flow rate of methane is 12sccm;
(5) Bonding:
and (3) sequentially placing the molybdenum table, the copper foil and the carbonized diamond into MPCVD equipment from bottom to top, wherein the carbonized layer is contacted with the copper foil, and bonding for 1.5 hours at 1000 ℃ in a plasma environment to obtain the single crystal diamond seed crystal bonded with the heat conduction copper foil, which can be used for growing low-stress single crystal diamond.
(6) Deposition and growth:
FIG. 6 is an optical photograph of a single crystal diamond grown before the heat dissipation condition is improved without the method of the present invention in the prior art, wherein the surface shape of the diamond is uneven, convex-concave and surface-wrinkled are obvious, which indicates that the shape change caused by unstable crystallization and overlarge internal stress and lower crystal quality are caused by unstable growth process, FIG. 9 is a Raman spectrum diagram thereof, and the first-order Raman peak of the diamond is located at 1328.74 cm -1 With standard diamond first order raman peak 1332 cm -1 The difference is 3.26 cm -1 Also, it is indicated that there is a large tensile stress in the crystal.
FIG. 7 and FIG. 8 are optical photographs of single crystal diamond grown by the method of the present invention after improving heat dissipation conditions, wherein the diamond surface is smooth and regular, showing that the crystal quality is high and the internal stress is low during the growth process, FIG. 10 is a Raman spectrum of FIG. 7, and the first order Raman peak of the diamond is located at 1331.99 cm -1 The method comprises the steps of carrying out a first treatment on the surface of the FIG. 11 is a Raman spectrum of FIG. 8, with a first-order Raman peak of diamond at 1332.04 cm -1 The method comprises the steps of carrying out a first treatment on the surface of the Both approach the ideal characteristic peak 1322 and 1322 cm -1 The method shows that the single crystal diamond obtained by the method has good crystal quality and small internal stress, and has good toughness and difficult cracking when being applied in the later period, and the influence of the internal stress on the cutter is reduced.
In step (3) of the method, molybdenum plating may be replaced by tantalum plating, tungsten plating, titanium plating, or the like, as long as it is easily applicable to forming a metal carbide layer with diamond.
Claims (8)
1. A method for reducing stress during CVD single crystal diamond growth comprising the steps of:
(1) Cleaning
Cleaning the single crystal diamond seed crystal to be treated and the heat conduction copper foil, and drying to remove impurities;
(2) Seed etching
Etching and preprocessing the monocrystalline diamond seed crystal obtained in the step (1) in an oxyhydrogen plasma environment to obtain monocrystalline diamond seed crystal with larger surface roughness;
(3) Coating film
Plating molybdenum on the single crystal diamond seed crystal obtained in the step (2) through a plating process;
(4) Carbonization treatment
Carrying out surface carbonization treatment on the single crystal diamond seed crystal plated with the molybdenum layer obtained in the step (3) in a hydrogen and methane plasma atmosphere, so that a metal carbide layer is generated on the surface of the single crystal diamond seed crystal plated with the molybdenum layer;
(5) Bonding
Bonding the surface of the monocrystalline diamond seed crystal with the metal carbide layer obtained in the step (4) with the copper foil of the heat conducting layer in a plasma environment by a sample stage to obtain the monocrystalline diamond seed crystal bonded with the heat conducting copper foil;
(6) Deposition growth
And (3) placing the monocrystalline diamond seed crystal obtained in the step (5) into MPCVD equipment, and carrying out monocrystalline diamond deposition at high temperature to obtain the low-stress monocrystalline diamond under the same technological conditions.
2. A method of reducing stress during CVD single crystal diamond growth according to claim 1, wherein: in the step (1), single crystal diamond seed crystals are placed in aqua regia for 2 hours in a water bath at 80 ℃, then the seed crystals and the heat conduction copper foil after acid washing are respectively washed in acetone and absolute ethyl alcohol for 20 minutes in an ultrasonic mode, then the seed crystals and the heat conduction copper foil are washed in pure water for 5 minutes, and the seed crystals and the heat conduction copper foil are placed in an oven for drying.
3. A method of reducing stress during CVD single crystal diamond growth according to claim 1, wherein: and (2) etching the monocrystalline diamond seed crystal in the step under the condition of oxyhydrogen plasma, wherein the etching time t1 is more than or equal to 1h and less than or equal to 3h.
4. A method of reducing stress during CVD single crystal diamond growth according to claim 1, wherein step (3) is a magnetron sputter coating process.
5. A method of reducing stress during CVD single crystal diamond growth according to claim 3; the method is characterized in that the magnetron sputtering coating is performed under the vacuum condition that the pressure is not more than 0.001Pa, the magnetron sputtering time is t, t2 is not more than 10min and not more than 15min, and the magnetron sputtering power is 100W.
6. The method of reducing stress during CVD single crystal diamond growth according to claim 1, wherein the temperature of the carbonization treatment in step (4) is 700 ℃ to 800 ℃, the methane flow is 1% to 8% of the hydrogen volume flow, and the carbonization time is 0.5h to 2h.
7. The method of claim 1, wherein the sample stage of step (5) is bonded in a plasma environment at 900-1000 ℃ for a bonding time of not less than 1h.
8. A method of reducing stress during CVD single crystal diamond growth according to claim 1, wherein the single crystal diamond deposition temperature in step (6) is 850-950 ℃ and the deposition time is about 72-120 hours.
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